反応 #1838

ord-a19347c988eb4c1c9861adc66fd17858

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度while cooling
  2. 2
    温度The reaction mixture was heated at 50°-55° C. for 1 hour
  3. 3
    温度after cooling
  4. 4
    workup.ADDITIONwas poured onto ice
  5. 5
    ろ過the residue was filtered off with suction
  6. 6
    その他to give
  7. 7
    その他after drying
  8. 8
    その他8.8 g of product, melting point 90°-93° C. (sintering at 85° C.)

実験手順

29.7 ml of nitric acid were added dropwise to 76.5 ml of concentrated sulfuric acid, while cooling and stirring, and 9.0 g (43.7 mmol) of 3-trifluoromethoxybenzoic acid were then added. The reaction mixture was heated at 50°-55° C. for 1 hour and, after cooling, was poured onto ice, and the residue was filtered off with suction to give, after drying, 8.8 g of product, melting point 90°-93° C. (sintering at 85° C.).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05726305uspto-grants-1998_03